CN207775345U - Diamond/graphene composite heat conduction film and cooling system - Google Patents
Diamond/graphene composite heat conduction film and cooling system Download PDFInfo
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- CN207775345U CN207775345U CN201721418398.6U CN201721418398U CN207775345U CN 207775345 U CN207775345 U CN 207775345U CN 201721418398 U CN201721418398 U CN 201721418398U CN 207775345 U CN207775345 U CN 207775345U
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Abstract
The utility model provides a kind of diamond/graphene composite heat conduction film, including micron diamond film and graphene layer in micron diamond film surface is arranged.Diamond and graphene binding force are stronger in diamond/graphene composite heat conduction film, and have lower interface resistance between diamond and graphene, and diamond/graphene composite heat conduction film of formation has efficient heat conductivility.The utility model additionally provides a kind of cooling system.Cooling system includes heater element, radiator and heat conducting film, the heat conducting film includes diamond/graphene composite heat conduction film described above, the heat conducting film adheres between the heater element and the radiator, so that the heater element transfers heat to the radiator to radiate by the heat conducting film.The heat conducting film can pick up and be placed with, therefore be easy to industrialized production and use, while excellent radiation performance independently of heater element and radiating element individualism.
Description
Technical field
The utility model is related to heat conducting film fields, and in particular to a kind of diamond/graphene composite heat conduction film and system of radiating
System.
Background technology
Currently, diamond heat-sink piece and the composite material based on graphene are led in the heat management of high-end high power device
Domain is centainly applied, but in order to further increase the heat conductivility of material, bonded diamond and graphene are respectively in longitudinal direction
Become research hotspot with the higher advantage of lateral thermal coefficient.It is as " a kind of in disclosed in patent of invention CN201510406256.7
Superelevation orients the preparation method of heat conduction C-base composte material ", by the way that natural or artificially synthesizing diamond surface is carried out accurate throwing
Light, cleaning, reach atomically flating；Then the graphene for relying on polymethyl methacrylate (PMMA) substrate is directly tiled
Highly directional heat-conductive composite material is obtained in diamond surface.But it is to be transferred to the graphene for relying on PMMA substrates in the patent
On diamond, binding force is low between the graphene and diamond of acquisition, and interface cohesion is poor, and interface resistance is higher, preparation process
It is complicated.
Therefore, it is necessary to provide a kind of novel diamond/graphene composite heat conduction film.
Utility model content
To solve the above problems, the utility model provides a kind of diamond/graphene composite heat conduction film, in the brilliant gold of micron
The binding force of hard rock film surface setting graphene layer, the micron diamond film and the graphene layer is stronger and described
The good heat dispersion performance of diamond/graphene composite heat conduction film.
The utility model provides a kind of diamond/graphene composite heat conduction film, including micron diamond film and
Graphene layer in the micron diamond film surface is set.
Wherein, the graphene layer includes single-layer graphene or multi-layer graphene.
Wherein, the thickness of the graphene layer is 1-60 atomic thickness.
Wherein, the graphene layer includes the single-layer graphene for being laid in the micron diamond film surface.
Wherein, the graphene layer further comprises vertical-growth in the vertical graphene on the single-layer graphene.
Wherein, the vertical graphene is arranged in array.
Wherein, the thickness of the micron diamond film is 200 μm of -2mm.
Wherein, the crystallite dimension in the micron diamond is 1 μm -10 μm.
Wherein, the diamond/graphene composite heat conduction film further includes transition metal layer, and the transition metal layer is located at institute
State the side far from the graphene layer of micron diamond film.
Diamond provided by the utility model/graphene composite heat conduction film, diamond and graphene binding force are stronger, are formed
Excellent conductive structure, graphene are conducive to the high heat conductance in planar structure direction, and diamond is conducive to vertical
There is longitudinal high heat conductance of in-plane lower interface resistance, structure of composite membrane integrally to have between diamond and graphene
There is efficient heat conductivility.
The utility model additionally provides a kind of cooling system, including heater element, radiator and heat conducting film, the heat conduction
Film includes diamond/graphene composite heat conduction film described above, and the heat conducting film adheres on the heater element and dissipated with described
Between hot device, so that the heater element transfers heat to the radiator to radiate by the heat conducting film.
Cooling system provided by the utility model includes heat conducting film, and the heat conducting film can be independently of heater element and radiator
Part individualism can be picked up and be placed with, therefore be easy to industrialized production and use, while excellent radiation performance.
Description of the drawings
Fig. 1 is the structural schematic diagram for diamond/graphene composite heat conduction film that one embodiment of the utility model provides；
Fig. 2 is the structural schematic diagram for diamond/graphene composite heat conduction film that another embodiment of the utility model provides.
Specific implementation mode
As described below is preferred embodiments of the present invention, it is noted that for the ordinary skill of the art
For personnel, without departing from the principle of this utility model, several improvements and modifications can also be made, these are improved and profit
Decorations are also considered as the scope of protection of the utility model.
As shown in Figure 1, the utility model embodiment first aspect provides a kind of diamond/graphene composite heat-conducting
Film, including micron diamond film 1 and graphene layer 2 in the micron diamond film surface is set.
In the utility model embodiment, the crystal grain in the micron diamond is micron order.Optionally, the micron
Crystallite dimension in diamond is 1 μm -10 μm.Optionally, the thickness of the micron diamond film is 200 μm of -2mm.
Optionally, the micron diamond film can be the disk of a diameter of 20-50cm.Still optionally further, the brilliant gold of the micron
Hard rock film is the disk of a diameter of 25.4cm.In the utility model, graphene layer is set in micron diamond film surface,
Due to diamond film have high quality micron crystal structure, compare nanocrystalline diamond film, micron diamond film have compared with
High thermal coefficient.In addition, the size of the micron diamond film in the utility model embodiment is larger, can meet big
For the demand of large-area diamond/graphene composite heat conduction film in power electronic device.
In the utility model embodiment, the graphene layer includes single-layer graphene or multi-layer graphene.Optionally, institute
The thickness for stating graphene layer is 1-60 atomic thickness.As shown in Fig. 2, still optionally further, the graphene layer includes tiling
Single-layer graphene 21 on 1 surface of micron diamond film.The single-layer graphene is a carbon atom thickness
Two-dimensional reticulated film.It is the single-layer graphene that the single-layer graphene, which is laid in the micron diamond film surface,
Extending direction is parallel with the micron diamond film surface.Still optionally further, the graphene layer further comprises hanging down
Growing straight is longer than the vertical graphene 22 on the single-layer graphene 21.The i.e. described vertical graphene vertical-growth is in micron crystalline substance
Diamond film surface.Since vertical graphene has very high specific surface area, the effective of composite film surface can be improved and dissipated
Hot area.Still optionally further, the vertical graphene is arranged in array.Still optionally further, the thickness of the vertical graphene
Degree is 1-60 atomic thickness.Still optionally further, the graphene layer includes being laid in the micron diamond film table
The multi-layer graphene and vertical-growth in face are in the vertical graphene on the multi-layer graphene.
In the utility model embodiment, it is substrate through forming core that the graphene layer, which is using the micron diamond film,
It is obtained with growth.
In the utility model embodiment, the diamond/graphene composite heat conduction film further includes transition metal layer, described
Transition metal layer is located at the side of the separate graphene layer of the micron diamond film.Optionally, the diamond/
Graphene composite heat conduction film includes transition metal layer, micron diamond film and graphene layer, the transition metal layer successively
Positioned at the bottom of the micron diamond film.
Diamond/graphene composite heat conduction film that the utility model embodiment mode first aspect provides, micron crystalline substance Buddha's warrior attendant
Stone and graphene binding force are stronger, form excellent conductive structure, and graphene is conducive to improve in planar structure direction
High heat conductance, diamond is conducive to improve longitudinal high heat conductance in vertical plane direction, and between diamond and graphene
With lower interface resistance, structure of composite membrane integrally has efficient heat conductivility.
The utility model embodiment second aspect provides a kind of preparation side of diamond/graphene composite heat conduction film
Method, including：
S01 provides substrate, and micron diamond film is deposited in the substrate surface；
S02, substrate described in erosion removal, obtains the micron diamond film of self-supporting；Wherein, the self-supporting is micro-
Rice diamond film waits for forming core surface including one, described to wait for forming core surface for the micron diamond film and institute before corrosion
State the contact surface of substrate；
S03 waits for depositing transition metal layer on forming core surface that deposition is had to the micron of the self-supporting of transition metal layer described
Diamond film is placed in progress short annealing processing in heated filament vapor deposition chamber cavity, and it is multiple to obtain the diamond/graphene
Heat conducting film is closed, the annealing temperature is 800-1100 DEG C, and the annealing time is 1-5min.
In S01, the substrate includes monocrystalline silicon or metal substrate such as molybdenum, copper, iron etc..Optionally, the substrate is single
Crystal silicon substrate.Optionally, before preparing micron diamond film, first monocrystal silicon substrate is pre-processed, the pre- place
Reason operates：
Monocrystal silicon substrate is placed in NH4OH/H2O2/ deionized water (volume ratio 1:1:5) in mixed solution, 70 are heated to
DEG C -80 DEG C react 1-2 hour, and silicon chip is rinsed well, and then silicon chip is sequentially placed into acetone soln and is cleaned by ultrasonic 10-30 and divides
Clock, be cleaned by ultrasonic in deionized water 10-30 minutes and and alcoholic solution in be cleaned by ultrasonic 10-30 minutes.
In the utility model embodiment, before preparing the micron diamond film, the substrate is added
For strong forming core treatment process to improve the Enhancing Nucleation Density of diamond, the forming core treatment process includes that the substrate is placed in diamond
It carries out being ultrasonically treated or the substrate being placed in vapor deposition chamber in powder suspension carrying out bias reinforcement forming core processing.
Specifically, the substrate is placed in the operation being ultrasonically treated in bortz powder suspension includes：
Substrate is placed in nano-diamond powder suspension and is ultrasonically treated 1-3 hours.Optionally, the nano-diamond powder
The average grain diameter of the middle nano-diamond powder of suspension is 5nm.Optionally, the Zeta potential of the nano-diamond powder suspension
About ± 50mV.
Specifically, the substrate is placed in vapor deposition chamber carry out bias reinforce forming core processing operation include：
By taking HFCVD as an example, using double bias hot-wire chemical gas-phase depositions, apply just in heated filament upper gate in nucleation process
Bias, silicon base apply back bias voltage；For microwave plasma CVD, substrate applies back bias voltage.Methane ratio omits in nucleation process
Height, nucleation process is completed about after half an hour, closes grid bias power supply, adjusts methane concentration and other technological parameters to being suitble to select height
The condition of heat conduction micron diamond film growth.Specifically：HFCVD grid biases are+30V, and substrate bias is -150V；
Plasma CVD substrate bias is -150V.
After above-mentioned reinforcement forming core treatment process, the Enhancing Nucleation Density of the micron diamond film is more than 1010/
cm2。
In S01, after reinforcing forming core treatment process, micron diamond film is prepared in the substrate surface.It can
Selection of land, the preparation process are chemical vapor deposition, and the method for the chemical vapor deposition includes microwave plasma chemical gas
Mutually prepared by deposition (MPCVD) or hot-wire chemical gas-phase deposition (HFCVD).
Specifically, the design parameter of the HFCVD is as follows：
It is passed through gaseous carbon source and hydrogen carries out hot-wire chemical gas-phase deposition, air pressure 3000-5000Pa, heater power is
5000-8000W, base reservoir temperature are 500 DEG C -1000 DEG C, and sedimentation time is 100-300 hours.More specifically, heater array is by 9
The tantalum wire of a diameter of 0.5mm of root forms, and the spacing of heated filament and sample surfaces is 8mm, and methane/hydrogen flowing quantity is respectively 16sccm/
800sccm, total gas couette 816sccm, air pressure 4000Pa, heater power 7000W, base reservoir temperature are 900 DEG C, deposition
Time is 200 hours.
Specifically, the design parameter using microwave plasma CVD (MPCVD) is as follows：
It is passed through gaseous carbon source and hydrogen carries out microwave plasma CVD, air pressure 20-40Torr, microwave work(
Rate is 1000-1500W, and base reservoir temperature is 700-900 DEG C, and sedimentation time is 100-300 hours.More specifically, methane/hydrogen stream
Amount is respectively 2sccm/298sccm, total gas couette 300sccm, air pressure 30Torr, microwave power 1200W, substrate temperature
Degree is 850 DEG C, and sedimentation time is 200 hours.
In the above-mentioned technical solutions, the method for used growing diamond membrane except microwave plasma chemical gas phase it is heavy
Outside product and hot filament chemical vapour deposition method, direct current, radio frequency, hot cathode or injection plasma chemical vapor deposition can also be
Method etc. can grow any method of diamond.
In S02, micron diamond film obtained is detached from the substrate, obtains the micron diamond of self-supporting
Film.Optionally, the micro- of support is available from after corroding to the substrate by the mixed solution of hydrofluoric acid/sulfuric acid/glacial acetic acid
Rice diamond film.Or the micron diamond film of support is available from after corroding to the substrate by KOH solution.Tool
Body, the etching operation is：There is the substrate of micron diamond film to be placed in hydrofluoric acid/sulfuric acid/glacial acetic acid deposition
It is 1 by volume:1:Corroded in 2 mixed solutions formed；Or deposition is had to the substrate of micron diamond film
It is placed in 30% (w/v) KOH solution, is heated to 85 DEG C -100 DEG C and is corroded, etching time is 5-24 hours, will then be obtained
Free-standing diamond film clean, drying.After corrosion, formation waits for that the preceding diamond thin and institute (are corroded in forming core surface
State the contact surface of substrate) it is very smooth, it can be as the aufwuchsplate of high-quality graphene.Optionally, the forming core surface of waiting for
Surface roughness (rms, roughness)<1nm.
The utility model carries out the growth of graphene using diamond thin forming core face, provides an atomic-level flatness
Diamond surface, avoid the complicated technology chemically-mechanicapolish polished to coarse micron diamond film, while gold
Hard rock film has high quality micron crystal structure, compares the higher nanocrystalline diamond film of flatness, micron diamond film tool
There is higher thermal coefficient.
In S03, wait for depositing transition metal layer on forming core surface described.Specifically, by the brilliant gold of the micron of the self-supporting
Hard rock film is placed in electron beam deposition apparatus, is opened equipment to background vacuum and is reached 1 × 10-7-1×10-8Torr is opened
Electron beam adjusts electron beam high pressure and electric current, and it is 0.3-0.8nm/s, sedimentation time 15- to keep the deposition rate of transition metal
30s.Specifically, it opens equipment to background vacuum and reaches 10-8Torr opens electron beam, adjusts electron beam high pressure and electric current, protects
The deposition rate for holding transition metal is 0.5nm/s, sedimentation time 20s.
Optionally, the thickness that deposition obtains the transition metal layer before annealing is 1nm-50nm, the transition metal layer
Material includes nickel, copper, iron or cobalt.
In S03, after transition metal layer is prepared, there is the micron diamond of the self-supporting of transition metal layer thin deposition
Film is placed in progress short annealing processing in heated filament vapor deposition chamber cavity, obtains the diamond/graphene composite heat conduction film.
Optionally, sample is placed in HFCVD equipment, is rapidly heated short annealing similar with what is closed by heated filament
Journey can obtain the graphene forming core layer of high quality, should need to optimize process conditions in the process.Optionally, described to move back
The design parameter of fiery treatment process is：It is passed through protective gas and hydrogen in the heated filament vapor deposition chamber cavity, makes the chamber
Air pressure in body is 2800-3200Pa, the heated filament in the heated filament vapor deposition chamber cavity and the micron diamond film
The spacing on surface is 4-10mm, heater power 5000-7000W, the micron crystalline substance for depositing the self-supporting for having transition metal layer
The temperature of diamond thin is 800-1100 DEG C, soaking time 1-5min.Still optionally further, the protective gas is nitrogen
Gas, the protective gas are nitrogen, and the flow of nitrogen and hydrogen is 425sccm/75sccm, total gas couette 500sccm.Tool
Body, heater array is made of the tantalum wire of 9 a diameter of 0.5mm, and heated filament has the micron of the self-supporting of transition metal layer with deposition
The spacing of diamond film surface is 5mm, air pressure 3000Pa, heater power 7000W, and deposition has oneself of transition metal layer
The temperature of the micron diamond film of support is 1100 DEG C, soaking time 1min.
Optionally, it is that 30-50 DEG C/min is cooled to 200 DEG C -400 DEG C with rate after the annealing.Optionally, it moves back
It is that 40 DEG C/min is cooled to 200 DEG C -300 DEG C with rate after fire.
In annealing process, the transition metal layer constantly sink, until being down to a micron bottom for diamond film.It can
With understanding, there may be the transition metal particles of part to penetrate into the micron diamond film.
In the utility model embodiment, the utility model carries out the shape of graphene using hot-filament chemical vapor deposition equipment
Core and growth, compared to other short annealing treating methods, HFCVD can provide the atmospheric condition for being more suitable for graphene growth and
Plasma environment is conducive to the quality for improving graphene.Forming core and the growth of graphene, the process are induced with transition metal layer
In the carbon sources such as methane need not be added, in the transition metal-catalyzed micron diamond film in the transition metal layer
Part carbon forms graphene layer, realizes surface carbon atomic layer by diamond knot by the diffusion of diamond and transition metal layer
Structure changes to the self assembly of graphene-structured.
In the utility model embodiment, graphene layer obtained includes being laid in the micron crystalline substance Buddha's warrior attendant after annealing
The single-layer or multi-layer graphene of stone film surface.
In the utility model embodiment, graphene layer obtained includes being laid in the micron crystalline substance Buddha's warrior attendant after annealing
Then the single-layer graphene of stone film surface prepares vertical-growth in described described on single-layer graphene in accordance with the following methods
Vertical graphene on single-layer graphene：
After annealing, in the heated filament vapor deposition chamber cavity being passed through carbon-source gas is deposited, and vertical stone is obtained
Black alkene.Specifically growth parameter(s) is：It is passed through gaseous carbon source, hydrogen and argon gas and carries out hot-wire chemical gas-phase deposition, depositing temperature is
600-800 DEG C, air pressure 3000-6000Pa, power 5000-7000W, sedimentation time is 2-3 hours.Optionally, the gas
State carbon source includes C2H2、CH4、CF4、CHF3And C2F6In one kind.Optionally, specific growth parameter(s) is as follows：CH4、H2, Ar ratio
Example is 40%：40%：20%, air pressure 4000Pa, heater power 6000W, depositing temperature are 800 DEG C, sedimentation time 2h.
More specifically, argon gas/methane/hydrogen flowing quantity is 200sccm/400sccm/400sccm, total gas couette 1000sccm.
In the utility model embodiment, graphene layer obtained includes being laid in the micron crystalline substance Buddha's warrior attendant after annealing
Then the single-layer graphene of stone film surface continues described on single-layer graphene to prepare several layer graphenes in accordance with the following methods
To obtain multi-layer graphene：
After annealing, in the heated filament vapor deposition chamber cavity being passed through carbon-source gas is deposited, and multilayer stone is obtained
Black alkene.Specifically growth parameter(s) is：It is passed through gaseous carbon source, hydrogen and argon gas and carries out hot-wire chemical gas-phase deposition, depositing temperature is
800-1100 DEG C, air pressure 3000-6000Pa, power 5000-7000W, sedimentation time 1-1.5h.Optionally, the gas
State carbon source includes C2H2、CH4、CF4、CHF3And C2F6In one kind.Specifically, continue the growth of graphene in HFCVD,
Specific growth parameter(s) is as follows：Air pressure is 3000Pa, heater power 7000W.More specifically, nitrogen/hydrogen/methane flow is
410sccm/75sccm/15sccm, total gas couette 500sccm.
Substrate of the utility model using diamond thin forming core face as graphene growth contributes to smooth continuous high-quality
Amount graphene growth can obtain the graphene forming core layer of high quality by annealing process, and the preparation method is simply easily grasped
Make, diamond obtained/graphene composite heat conduction film thermal conductivity is higher.
The utility model embodiment third aspect provides a kind of cooling system, including heater element, radiator and
Heat conducting film, the heat conducting film include diamond/graphene composite heat conduction film as described in above-mentioned first aspect, the heat conducting film patch
It is placed between the heater element and the radiator, so that the heater element transfers heat to institute by the heat conducting film
Radiator is stated to radiate.
In cooling system provided by the utility model, diamond/graphene composite heat conduction film compared to diamond heat dissipation film,
The heat conductivility in plane greatly improved in thermal conductivity higher, especially graphene, by the way that the high density hot-fluid of heat point source is fast
Speed diffuses in entire plane, reduces the heat flow density into diamond first, then by diamond film horizontal and/or
Vertical direction exports hot-fluid, and heat dissipation performance greatly improved.
Above-described embodiments merely represent several embodiments of the utility model, the description thereof is more specific and detailed,
But it should not be understood as limiting the scope of the patent of the utility model.It should be pointed out that for the common of this field
For technical staff, without departing from the concept of the premise utility, various modifications and improvements can be made, these all belong to
In the scope of protection of the utility model.Therefore, the protection domain of the utility model patent should be determined by the appended claims.
Claims (7)
1. a kind of diamond/graphene composite heat conduction film, which is characterized in that including micron diamond film and be arranged in institute
A micron graphene layer for diamond film surface is stated, the graphene layer includes being laid in the micron diamond film table
The single-layer or multi-layer graphene and vertical-growth in face are in the vertical graphene on the single-layer or multi-layer graphene.
2. diamond as described in claim 1/graphene composite heat conduction film, which is characterized in that the thickness of the graphene layer
For 1-60 atomic thickness.
3. diamond as described in claim 1/graphene composite heat conduction film, which is characterized in that the vertical graphene is in battle array
Row arrangement.
4. diamond as described in claim 1/graphene composite heat conduction film, which is characterized in that the micron diamond is thin
The thickness of film is 200 μm of -2mm.
5. diamond as described in claim 1/graphene composite heat conduction film, which is characterized in that in the micron diamond
Crystallite dimension be 1 μm -10 μm.
6. diamond as described in claim 1/graphene composite heat conduction film, which is characterized in that the diamond/graphene is multiple
It further includes transition metal layer to close heat conducting film, and the transition metal layer is located at the separate graphite of the micron diamond film
The side of alkene layer.
7. a kind of cooling system, which is characterized in that including heater element, radiator and heat conducting film, the heat conducting film includes power
Profit requires 1-6 any one of them diamond/graphene composite heat conduction film, the heat conducting film to adhere on the heater element and institute
Between stating radiator, so that the heater element transfers heat to the radiator to radiate by the heat conducting film.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109722641A (en) * | 2017-10-30 | 2019-05-07 | 深圳先进技术研究院 | Diamond/graphene composite heat conduction film and preparation method thereof and cooling system |
| CN109825815A (en) * | 2019-02-21 | 2019-05-31 | 江西科技师范大学 | A kind of preparation method reducing diamond/copper heat-conductive composite material interface resistance |
| CN111356329A (en) * | 2018-12-21 | 2020-06-30 | 惠州昌钲新材料有限公司 | Thin high-conductivity heat-dissipation composite material with low interface thermal resistance |
| CN113461439A (en) * | 2020-03-30 | 2021-10-01 | 北京石墨烯研究院 | Graphene-ceramic composite material and preparation method and application thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109722641A (en) * | 2017-10-30 | 2019-05-07 | 深圳先进技术研究院 | Diamond/graphene composite heat conduction film and preparation method thereof and cooling system |
| CN109722641B (en) * | 2017-10-30 | 2023-09-22 | 深圳先进技术研究院 | Diamond/graphene composite heat conducting film, preparation method thereof and heat dissipation system |
| CN111356329A (en) * | 2018-12-21 | 2020-06-30 | 惠州昌钲新材料有限公司 | Thin high-conductivity heat-dissipation composite material with low interface thermal resistance |
| CN109825815A (en) * | 2019-02-21 | 2019-05-31 | 江西科技师范大学 | A kind of preparation method reducing diamond/copper heat-conductive composite material interface resistance |
| CN113461439A (en) * | 2020-03-30 | 2021-10-01 | 北京石墨烯研究院 | Graphene-ceramic composite material and preparation method and application thereof |
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